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A kind of preparation method of divalent metal iron-based spinel

A bivalent metal and spinel technology, applied in chemical instruments and methods, iron compounds, nickel compounds, etc., can solve the problems of easy agglomeration in the calcination process, difficult mixing of oxygen carriers, expensive reagents, etc., and achieve good high temperature Stability and mechanical stability, not easy to agglomerate, beneficial to recycling and utilization

Active Publication Date: 2020-04-14
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the preparation methods of mechanical mixing, impregnation, and freezing granulation are simple, it is difficult to fully mix the components of the oxygen carrier; the reagents used in the sol-gel method are expensive, the preparation time is long and the operation process is complicated; the alcohol-salt hydrolysis method requires expensive Alcohol salts, the production cost is extremely high
Co-precipitation method is simple and easy to operate, but it is easy to agglomerate during calcination

Method used

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  • A kind of preparation method of divalent metal iron-based spinel
  • A kind of preparation method of divalent metal iron-based spinel
  • A kind of preparation method of divalent metal iron-based spinel

Examples

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Embodiment 1

[0037] A kind of nano-nickel-iron spinel (NiFe 2 o 4 ) preparation method, comprising the following steps:

[0038] 1) Prepare 300mL of solution A, in which the molar ratio of Ni / Fe is 1:2, Ni 2+ Concentration is 0.1mol / L, Fe 3+ The concentration is 0.2mol / L; prepare 200mL of ammonium carbonate solution with a concentration of 0.5mol / L.

[0039] 2) Add 0.5mol / L ammonium carbonate solution at 5mL / min to solution A with a magnetic stirring speed of 600r / min. The initial pH of solution A before adding ammonium carbonate solution is 0.8, and the pH of the mixed solution after adding is 2.8 Left and right, the solution turns into a paste-like suspension, and after the magnetic stirring lasts for 30s, an aqueous sol with a certain solid structure is formed.

[0040] 3) Slowly dry the hydrosol in a drying oven at 105°C for 6 hours to form a transparent block-shaped dry gel; then place the dried gel in a covered crucible and heat it at 400°C for 2 hours in a muffle furnace to isol...

Embodiment 2

[0044] A kind of nano-magnesium iron spinel (MgFe 2 o 4 ) preparation method, comprising the following steps:

[0045] 1) Prepare 500mL of solution A, in which the molar ratio of Mg / Fe is 1:2, Mg 2+ Concentration is 1mol / L, Fe 3+ The concentration is 2mol / L; prepare 500mL of ammonium carbonate solution with a concentration of 1mol / L.

[0046] 2) Put 1mol / L ammonium carbonate solution 10mL / min into solution A with a magnetic stirring speed of 800r / min. The initial pH of solution A before adding ammonium carbonate solution is 0.01, and the pH of the mixed solution after adding is about 2. It becomes a paste-like suspension, and after magnetic stirring lasts for 60s, a hydrosol with a certain solid structure is formed.

[0047] 3) Slowly dry the hydrosol in a drying oven at 105°C for 12 hours to form a transparent block-shaped dry gel; then place the dried gel in a covered crucible and heat it at 350°C for 12 hours in a muffle furnace to isolate the air. It will be decompose...

Embodiment 3

[0051] A kind of nano copper iron spinel (CuFe 2 o 4 ) preparation method, comprising the following steps:

[0052] 1) Prepare 300mL of solution A, in which the molar ratio of Cu / Fe is 1:2, Cu 2+ Concentration is 0.5mol / L, Fe 3+ The concentration is 1mol / L; prepare 200mL of ammonium carbonate solution with a concentration of 2mol / L.

[0053] 2) Put 1mol / L ammonium carbonate solution 15mL / min into solution A with a magnetic stirring speed of 600r / min. The initial pH of solution A before adding ammonium carbonate solution is 0.5, and the pH of the mixed solution after adding is about 2.5. It becomes a paste-like suspension, and after magnetic stirring lasts for 30s, a hydrosol with a certain solid structure is formed.

[0054] 3) Slowly dry the hydrosol in a drying oven at 85°C for 12 hours to form a transparent block-shaped dry gel; then place the dried gel in a covered crucible and heat in a muffle furnace at 500°C for 2 hours in isolation from the air. It will be decompo...

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Abstract

The invention provides a preparation method of divalent metal iron-based spinel. The preparation method comprises the steps as follows: S1, mixing a ferric nitrate solution and a divalent metal nitrate solution in the solute mole ratio being 1:2 to obtain a solution A; S2, dropwise adding an ammonium carbonate or ammonium bicarbonate solution to the solution A to obtain a hydrosol solution; S3, drying the hydrosol solution obtained in the S2 at 65-105 DEG C, and performing forming at 350-550 DEG C to obtain a spinel precursor; S4, calcining the spinel precursor at 700-1,100 DEG C to obtain divalent metal iron-based spinel, wherein no continuous foam exists in the solution when ammonium carbonate or ammonium bicarbonate is dropwise added. The method has a simple and quick process, the requirement for equipment and the preparation cost are reduced, the conditions are easy to control in the preparation process, and mass production can be realized. Meanwhile, divalent metal iron-based spinel with good crystal structure, particle size uniformity, high-temperature stability, mechanical stability and good magnetism can be obtained.

Description

technical field [0001] The invention belongs to the field of material preparation, and more specifically relates to a method for preparing divalent metal iron-based spinel. Background technique [0002] Mixed metal oxides, especially of the general formula AB 2 o 4 The spinel is a material with important application prospects. Because of their advantages of high magnetic permeability and low hysteresis loss, they are widely used in mutual inductance devices, magnetic core bearings, transfer switches, and magnetic recording. Recently, studies have shown that oxygen-deficient iron-based spinel has very good redox activity as an oxygen carrier, and has great potential in chemical chain cycle reactions. In addition, its good magnetic properties make it easier to Separated from other materials and reused many times. [0003] Most of the currently studied oxygen carriers are transition state metal oxides. Among these oxides, iron oxide as an oxygen carrier has a slightly lowe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G53/00C01G49/00C01G3/00
CPCC01G3/00C01G49/0036C01G49/0081C01G53/00C01P2002/32C01P2004/52C01P2004/82C01P2006/42
Inventor 许细微孙焱蒋恩臣王明峰任永志胡志锋王家旻李志宇
Owner SOUTH CHINA AGRI UNIV
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